Hydrogenating oils, fats, and fatty acids, &amp;c.



J. N. HUMPHREYS. HYDROGENATING OILS, FATS, AND FATTY ACIDS, 6w. APPLICATION FILED FEB.28,1913.

1,100 735. Patented June 23, 1914.

Quinn H501 JERQME N. l1

rnanrsl, or DALLAS, arenas.

HYIDJRUGENATKNG @1138, WATS, AND ll'h'llhY ACJEDE, etc.

specification of Letters Patent.

Patented dune bid, rare,

Application flied February as, 1918. herbal Ito. #591,353?

/ marked thereon.

tit

' through, for

This invention relates to the saturating oi v acids and their glycerids and other eocta, with hydrogen in the presence of in, y divided catalytic agents, the reaction tolrowingalong well known lines as developed by Sabatier and Senderens, Paalg lltoth, Ratlritin, lmpatiew, Norman, @rosfield, Kayser and others, The said investigators in this art, have rop'osed various methods of handling the oi s, etc., and exposing the same to the action of hydrogen, as, for example, it has been proposed to spray the oil from a nozzle into an atmosphere of hydrogen, to bubble the h drogen through a pool of the oil, to propc the oil and catalytic material into an atmosphere of hydrogen by mechanical agitators, and to repeatedly pass the oil through and over, or in contact with a static catalytic agent, usually a catalyzing metal held by a more or less p'orous carrier or a carrier having1 numerous passa es theret e body to be h rogenated and'the hydrogen gas by whic saturation is etlected. It has also been proposed to pass the hydrogen rapidly in or through the medium to be hydrogenated, and usually carrying comminuted catalyzing agents, with the idea that such rapid movement faciliw tated absorption. My own investigations lead me, however, to t e conclusion that the rapidity of the as movement, excepting only to increase t e amount of surface exposed, bears no relation tothe absorption nor to the rate of absorption, that is to say, a

elevation somewhat diagrammatic in charthe absorption is neither retarded nor accelerated save for the increase in the area of surface exposed, v

The objects of my presentinvention are to im rove upon the methods heretofore propose and practised, and to provide a more rapid process by enposin the o l, eta, carrying in suspenswn a fine y divided catalytic b ey more edectually' to; the action-oi the hydrogen gas, and in such manner as to avoid difiiculties heretofore encountered in the handling of the gas and oil, etc., to efi ec- I tuate the absorption process.

- Generally speaking, the invention contemplates the employment of a bed of hydro gen maintained under a reasona le pressure and the en osure in said body of hydrogen of thin un roken flowing films oi oils, etc, carrying in suspension finely divided catalyzing agents, the films of oil being maintained as thin as practicable without destroying their character as films or their capacity to flow in unbroken strata, towhich ends, oil, etc, having in suspension therein the finely divided catalyzing agent, is caused to flow over plane, slightly inclined, supporting surfaces in the hydrogen atmosphere aforesaid, and in the practical development of the invention it is caused to repeatedly flow over such supporting surfaces whereby any desired degree of saturation may be efilected, the whole operation bein conducted at a temperature suliiciently big to insure the maintenance of the material bein acted on in a sufliciently fluid condition to ow by gravity over the supporting surfaces in the I thin unbroken films referred to.

Competent apparatus for carryi the present invention into practice embo ies a closed chamber having within it plane, slightly. inclined, supporting plates, one above the other,aand successively discharging at their loweredges onto the u per portions of the next succeeding p ate with means at the bottom oi the chamber for collecting the material being acted upon and delivering the same to a suitable, pump or other means whereby it may be conveyed back to the top of the chamber to thereby complete the path of circulation, also means for eating the chamber, means for the introduction of hydrogen into the same, and 'for the introduction of fresh sup lies oil catalyzing material and oil, etc, to e satu- The accompanying drawing is a sectional actor, of an apparatus competent for carrying the present invention into practice, and .m said drawing reference numeral 1 1nd1- cates a cylindrical tanlr or chamber having a conical bottom 9 and preferably having an I upwardly dished top, The chamber or tank is surrounded by a heating jacket 2 which may be adapted for the circulatipn of steam I or other heating medium in the well known way. Within the chamber and ranging from top to bottom are a series of plane slightly inclined plates 5, 6, 7 etc., the upper plates, each at their lower edges, discharging onto the upper portions of the lower plates and proximate plates being incl ned in opposite directions, the'angle of inclination being such as is best calculated to cause a steady uniform and unbroken film of the material to be saturated, to flow down over the upper surfaces of the succeeding plates and the spaces at the discharge edges of the plates affording ample communicating passage ways to insure the uniform distribution of the atmosphere within the tank, or chamher. The pipe connection 20 at the bottom of the tank is provided with valves or gates 16 and 17, and a pipe 11 communicates with the pipe 20 between said valves or gates. Pipe 11 leads to a circulating pump 10 having its discharge through a pipe 12 extending up to. the top of the tank or chamber and entering the same through a nipple or.

coupling 3. Within the tank or chamber and receiving the discharge from the circulating pump is a distributing trough 4, preferably having a perforated bottom so as to give a uniform distribution over the upper portions of the topmost baffle plate. A hydrogen inlet 1a is provided and the hydro gen is admitted, preferably through a regulating valve 15, whereby the pressure in the hydrogenizing chamber may be maintained with uniformity to secure the best results. In practice about four atmospheres of pres sure has been found most suitable, all condition being taken into consideration.

In addition to the connections described, the chamber is also preferably provided at the top with a suitable admission opening 13 for the catalyzing agent and a blow-off cock 21 through which the gases coming from the chamber may be discharged when the chamber is initially filled with hydrogen, while the circulating system or the pipe communicating with the bottom of the chamber is provided with a test cock 18 through which samples of the saturated materials may be withdrawn for determining when the saturation has progressed to the desired degree.

Briefly, with an apparatus such as described, the process is carried out as follows; The pipe 20, being in communication with a supply of oil or other material which it is desired to hydrogenate, the valve 16 is opened and a sufficient quantity of the material is-pumped into the circulating system and to fill the conical bottom to a point where the outlet will be covered. The proper amountmay be determined by previous' measurement, if so desired. The valve 16 is then closed and valve 17 opened, whereupon the circulation of the material through the pump to the top of the chamber, thence in thin supported films to the bottom of the chamber and back to the pump. Sufficient hydrogen is admitted to flush out all other gases and the catalyzcr is then introduced through the opening 13 above the upper bafiie plate and which catalyzer, it is obvious, will become thoroughly mixed and intermingled with the liquid. The contents of the tank are kept at the proper temperature, usually about 300 F. and the supply of hydrogen being constant and under a reasonable pressure in the chamber, absorption rapidly ensues due to the larger surface of the catalytic carrying material exposed and its rapid change of surface accomplished by its flowing over its supporting surface, whereby fresh molecules are successively brought together at each. portion of the movement. 1

The operation is maintained and hydrogen is admitted until the desired degree of absorption is attained, which result may be determined from samples drawn from time to time through the test cock 18, the degree of absorption being indicated by the iodin number or titre of the fatty acid of the A y f 7 -material being hydrogenated.

it will be noted that by exposing thin unbroken supported films or streams of the material to be hydrogenizcd carrying in suspension the catalytic agent, a much larger proportion of the molecules of the material may be exposed. to the hydrogen, and for longer periods of time within a given area than in any other way, and the ellieacy of the invention is thought to be largely due to this fact, although, by causing the mate rial to flow over supporting surfaces there is a constant interchange and llllZQlCOllll11l1l gling' throughoutnll of the surface areas whereby fresh molecules are brought into contact with each other and into contact with the pervading hydrogen atmosphere, and to this action there may be attributed an eficiency not otherwise obtained.

While a cylindrical tank or chamber has been referred to herein, it is obvious that the particular shape of the chamber employed is not important or essential'to the I invention, and hence I do not wish to be limited to any particular form or dimension. Having thus described my invention what 1' claim as new and desire to secure by Let. ters Patent of the United States, is:

. 1. A process of hydrogcnating unsaturated fatty material, which consists in causing a mixture of the unsaturated fatty material and a divided catalytic agent to move in a film relatively slowly and quietly in a circuitous path in contact with a stationary inactive substance, in an atmosphere containing hydrogen.

2. A process of hydrogenating unsaturatedfatty material which consists in causing a mixture of the unsaturated fatty material and a pulverulent catalytic agent in a film of some inactive substance, in the presence of hydrogen.

3. A process of hydrogenating unsaturated fatty material, which consists 1n causing a mixture of the unsaturated fatty material and a finely divided catalytic agent in a film to flow quietly in a circuitous path repeatedly over and in contact with a smooth baffle element formed of some inactive substance, in an atmosphere containing hydrogen.

4. A process of hydrogenating unsaturated fatty material which consists in causing a mixture of the unsaturated fatty material and a divided catalytic agent to gravitate over inactive material of a relatively large area for prolonging the time of the travel of said mixture over and in contact with the inactive material, in the presence of hydroen. g 5. A process of h drogenating unsaturated fatty material,w ich consists in-causing a mixture of the same and a divided catalytic agent to flow without violent agitation .ove'r inactive material of a relatively large area, in the presence of an atmosphere containing hydrogen.

6. A process of h drogenating unsaturated fatty material, w ich consists 1n causing a mixture of the unsaturated fatty material and a divided catalytic agent,'in the form of a film, to flow over inactive'material, in the presence of an atmosphere containing. hydrogen.

7 A process of h drogenating unsaturated fatty material, wliich consists in causing a mixture of the unsaturated fatty material and a divided catalytic agent, in the form. of

a film, to flow by ravity over inactive material without vio ent agitation, in an atmosphere containing hydrogen. 7

8. A process of hydrogenating unsaturated fatty material, which consists in causing a mixture of the unsaturated material and a finely divided catalytic agent in the form of a film to move slowly and quietly without violent agitation, solely by gravitation, over and in contact with a stationary bafile ele-- ment of considerable area whereby the length of time consumed in. the travel of the film over the baflle element is prolonged in the presence of an atmosphere of hydro en.

9. The process of hydrogenatmg OllS, fats, fatty acids, etc., containing unsaturated constituents and carrying in suspension a finely divided catalyzing agent, which consists in exposing thin supported and flowing films of the material to gaseous hydrogen in a heated chamber.

10. A process of hydrogenating oils, fats,

fatty acids, etc., containing unsaturated constituents and carrying in sus ension a finely fats, fatty acids, etc., containing unsaturated constituents, which consists in exposing the material in-a series of succeeding thin supported unbroken flowing films to'the action of gaseous hydrogen while subjected to heat 'and pressure and in'commingling with the material to be hydrogenated acomminuted catalyzing agent.

: 13. The process of hydrogenating oils, fats, fatty acids, etc., containing unsaturated constituents and carrying in suspension a ,finely divided catalyzing agent which consists in flowing sa1d material by gravity over plane, inclined, supporting surfaces ar-' ranged in succession and exposed to an atmosphere of gaseous hydrogen and heat and in'circulating the material discharged from the lowermost support back to and depositing the same upon .the uppermost support.

JEROME N. HUMPHREYS.

Witnesses FRED G. TONGUE, E. H. KIRK. 

